CN104130138B - The continuous ammonification production technique of a kind of 2,4-dinitraniline - Google Patents
The continuous ammonification production technique of a kind of 2,4-dinitraniline Download PDFInfo
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Abstract
Invention describes the continuous ammonification production technique of a kind of 2,4-dinitraniline, with DNFB, ammoniacal liquor for raw material, temperature 160 DEG C ~ 170 DEG C, pressure reacts under 0.5MPa ~ 1.0MPa condition, and raw material is added ammoniation reactor continuously; After exceeding discharge port, material is successively from flowing to two auxiliary reactors, and it is 160 DEG C ~ 170 DEG C that temperature of reaction controls, and it is 0.5 ~ 1.0MPa that reaction pressure controls, and the ammoniation reactor reaction times is 42 minutes, and every platform auxiliary reactor reaction times is 15 minutes.The high and low energy consumption of this patent production efficiency, environmental protection, economy, labour intensity are low, safety, make full use of the waste heat of aminating reaction process, reclaim simultaneously and obtain by-product ammonium chloride, do not produce waste water, green production, good in economic efficiency.
Description
Technical field
The present invention relates to a kind of Chemical Engineering Technology, particularly the continuous ammonification production technique of a kind of 2,4-dinitraniline.
Background technology
2.4-dinitrochlorobenzene and ammoniacal liquor are raw material, preparation 2, the reaction principle of 4-dinitraniline is: with 2.4-dinitrobenzene 2,4-dinitrochlorobenzene, ammoniacal liquor are raw material, 2 are generated through amination reaction, 4-dinitraniline, this aminolysis reaction belongs to bimolecular nucleophilic substitution, first be the carbon atom generation nucleophilic attack be connected with chlorine atom on aromatic ring with the amino molecule of non-share electron pair, obtain the middle affixture with polarity, this middle affixture changes into rapidly reaction product 2,4-dinitraniline and by-product ammonium chloride.
At present, existing and once had about 2, it is all be interrupted single still to produce that 4 dinitranilines are produced, and production efficiency is low, long reaction time, produce pollute large.Demand for aminating reaction once designed many outstanding technical schemes, as being declared by Research Inst. of Petroleum Processing, SINOPEC of on 03 15th, 1989 Chinese State Intellectual Property Office bulletins, Authorization Notice No. is CN87105833.2, utility model patent title be the patent of invention of aminating reaction catalyst, its technical scheme adopted still has some deficits, it is also difficult to solve continuous seepage, the shortcoming of green production.
Summary of the invention
Technical problem to be solved by this invention is to provide the continuous ammonification production technique of a kind of 2,4-dinitraniline, low to solve interruption production efficiency, pollutes large, the technical problem that cost is high.
In order to realize the object solved the problems of the technologies described above, present invention employs following technical scheme:
The continuous ammonification production technique of a kind of 2,4-dinitraniline of the present invention, with DNFB, ammoniacal liquor for raw material, generates 2,4-dinitraniline, it is characterized in that:
With volume pump, DNFB, 18% ammoniacal liquor, water of condensation three kinds of raw materials are added reactor and continuously add main reactor by main reactor charging opening, wherein, the add-on of ammoniacal liquor and water makes DNFB: the NH contained in ammoniacal liquor
3mol ratio=1:(3.8 ~ 4.5 of amount), and NH
3: quality ratio=1:(4.3 ~ 4.6).
Main reactor is aminating reaction still, and aminating reaction still adopts the self-priming turbine stirring of double-suction head; The structure of self-priming turbine agitator is: arrange two pieces of circular cover plates respectively in the disc turbine agitator top and bottom meeting HG/T3796.5-2005 that the backward inclined type of impeller by 8 standards forms, and opens several pass into circular hole in tubular shaft at agitator axle sleeve position; Stirring rake lower end position is provided with current stabilization ring.According to the volume determination feed rate of main reactor, average residence time of material is made to be 35-50 minute; Further preferred, the structure that aminating reaction still adopts is: the agitator of aminating reaction still is made up of tubular shaft and double-suction head closed type turbine stirring rake, tubular shaft upper and lower opening, makes gaseous phase materials that reactor is sent out and below stir opening UNICOM; Double-suction head closed type turbine stirring rake by two groups of back-to-back combinations of closed type turbine agitator together, is opened multiple circular hole passed in tubular shaft at agitator axle sleeve position, stirring rake lower end position is provided with current stabilization ring; Aminating reaction still is temperature 160 DEG C ~ 170 DEG C, and pressure reacts under 0.5MPa ~ 1.0MPa condition;
After main reactor material exceedes the discharge port of aminating reaction still, material flow at least the first auxiliary reactor successively certainly, the second auxiliary reactor reacts; The mean residence time of material in every platform auxiliary reactor is 15 minutes; The number of auxiliary reactor is determined according to material reaction speed, as qualifiedly in material in the second auxiliary reactor does not just need the 3rd auxiliary reactor;
Utilize hot water pump to add water to coil pipe in main reactor, thus to main reactor cooling, make the temperature of main reactor control at 160 DEG C ~ 170 DEG C; Hot water out becomes steam afterwards from main reactor coil pipe, after steam is collected by sub-cylinder, for evaporation concentration section rapid steamer; Phlegma after evaporative condenser again collect return hot water pump continue cooling to main reactor utilize;
The temperature of reaction of two auxiliary reactors is controlled to be 160 DEG C ~ 170 DEG C, by the variable valve after surge tank, reaction pressure is controlled to be 0.5 ~ 1.0MPa, reacted material is through cooling row pressure, temperature is reduced to 60 ~ 70 DEG C, pressure reduces to normal pressure, form solid-liquid mixture, solid-liquid mixture is after centrifuge washing, and solid materials enters wrapping machine and carries out finished product packing.
Concrete further, after centrifugal 2, 4-dinitraniline mother liquor adds in rapid steamer, temperature 80 ~ 90 DEG C, vacuum overbottom pressure is evaporation concentration under the condition of below 0.05Mpa, to collect from being newly used for aminating reaction in water evaporates to mist collector in unsaturated ammonium chloride solution, the supersaturation ammonium chloride solution be left in rapid steamer utilizes the density in online Density Measuring Instrument detection rapid steamer, control ammonium chloride relay pump flow by density domination in rapid steamer at 1.0 ~ 1.1g/ml, utilize ammonium chloride relay pump by 2, 4-dinitraniline mother liquor is delivered to cooling down in ammonium chloride cooler, crystallization, material after crystallization is transported to whizzer and carries out centrifugation, obtain ammonium chloride product and the ammonium chloride mother liquor containing a small amount of ammonium chloride.
Average residence time of material described in this patent, be main reactor and auxiliary reactor useful volume in, material fill it up with the time.Namely under whipped state, the discharge port of main reactor and auxiliary reactor is as the criterion, the reactor volume determined, the time needed for this reactor volume filled it up with by material.
Concrete further, the structure of described main reactor be 3 charging openings on the end socket of main reactor upper end, discharge port is at the upper end of main reactor side kettle, and rinse mouth is established in bottom, main reactor has agitator, machine seal and step-down gear.
Concrete further, the mother liquor of described reacted material after centrifugal flows into 2,4-dinitraniline mother liquid tank.
Concrete further, the structure of described auxiliary reactor is: the charging opening of auxiliary reactor is 1/10th places of barrel lenght from the distance of end socket in kettle upper end, auxiliary reactor side, export in the upper end of auxiliary reactor side cylindrical shell from 1/9th places that the distance of end socket is barrel lenght, this charging opening and outlet angle in the vertical direction upper angle are 90 degree, rinse mouth is established in bottom, auxiliary reactor there is agitator, machine envelope and step-down gear; The stirring of auxiliary reactor is pusher stirring, the Main Function of auxiliary reactor extends the material reaction times, there is the material of a small amount of (less than 5%) could not react in main reactor, and then flow in auxiliary reactor proceed reaction, thus arriving qualified product, auxiliary reactor is provided with jacket heat-preservation.
Ammonium chloride mother liquor can flow into ammonium chloride mother liquor storage tank, or is delivered to rapid steamer again, continues in rapid steamer, continue evaporation and is separated reach ammonium chloride.
Preferred further, surge tank can be set after the second auxiliary reactor.Simultaneously the effect of surge tank to make ripe machine reacted material out maintain the pressure of main reaction machine and ripe machine by variable valve floating tank liquid level after surge tank, flows into cooler and carry out cooling row pressure.
This patent, by adopting distinctive structure of reactor and technical process, realizes wastewater zero discharge, and energy recovery utilizes.
These technical schemes also can combine mutually or combine, thus reach better technique effect.
The various content of the art of this patent scheme and ratio, if no special instructions, be mass content and ratio.
By adopting technique scheme, the present invention has following beneficial effect:
The one 2 of this patent, the continuous ammonification production technique of 4-dinitraniline, have the high and low energy consumption of production efficiency, environmental protection, the feature that economy, labour intensity are low, safe, technique effect is: this production line makes full use of the waste heat of aminating reaction process, by the waste water evaporation concentration containing ammonium chloride after ammonification, after the vapor condensation after evaporation, be reused for aminating reaction, reach the object of no effuent discharge, reclaim simultaneously and obtain by-product ammonium chloride, improve the economic benefit of this production line.
The waste gas discharged in production process absorbs through ammonia absorption device, and the gas after absorption reaches discharging standards, and the weak ammonia after absorption is reused for aminating reaction.
This production line only consumes a small amount of steam when driving, and for the intensification of reacting, after proceeding to continuous seepage, utilizes id reaction heat to maintain stable process conditions, and unnecessary reaction heat is used for later stage wastewater treatment, reduce the consumption of the energy in wastewater treatment process.
This production line production capacity is large, and continuously feeding and discharging, make full use of equipment, improves the utilization ratio of equipment.
Mother liquor after centrifugal is in rapid steamer, under certain vacuum degree condition, utilize aminating reaction heat to be concentrated by mother liquid evaporation, the steam after evaporation is reused for ammonification operation after condensation, and the mother liquor after concentrated is through cooling, by-product ammonium chloride crystallization, form solid-liquid mixture, solid-liquid mixture is after centrifugal, and ammonium chloride is packed, mother liquor after centrifugal sends into rapid steamer evaporation concentration again, realizes the zero release of production line waste water.
2,4-dinitraniline finished products of preparation consist of 2,6-dinitraniline about 1%, 2,4-dinitraniline about 98%, p-Nitroaniline about 0.05%.Quality control requirement is 2,4-dinitrobenzene amine contents 99.5% ~ 99.91% in 2,4-dinitrobenzene amine content 98% ~ 99%, second auxiliary reactors in 2,4-dinitrobenzene amine content 90% ~ 98%, first auxiliary reactors in amination machine.
And adopting common interrupter method to prepare 2,4-dinitranilines, its labor strength is large, and safety performance is unstable, increasing temperature and pressure, all leans on Artificial Control, and plant factor is low, has reinforced, reaction, insulation, cooling, discharging etc. to operate all holding times.Per ton 2 are produced in batch technology, 4-dinitraniline 2,4 dinitrochlorobenzene consumptions 1156.36 kilograms, 18% ammoniacal liquor consumes 1221.23 kilograms, adopt this patent production method in per ton 2,4-dinitraniline 2,4 dinitrochlorobenzene consumptions 1134.29 kilograms, 18% ammoniacal liquor consumption 1110.28 kilograms, compared with interruption production technique, adopt 18% ammoniacal liquor consumption of the method dinitraniline per ton of this patent to decline about 9%, throughput can reach 1.5 ~ 3 times of a breaking process.
Accompanying drawing explanation
Fig. 1 is the continuous ammonification production technological process of 2,4-dinitraniline of the present invention.
In Fig. 1, describe with ammoniacal liquor and DNFB as the process flow sheet of product 2,4-dinitraniline and byproduct ammonium chloride to be produced by raw material by some major equipments.
Fig. 2 is 2,4-dinitraniline synthesis schematic diagram.Ripe machine and auxiliary reactor in figure.
Fig. 3 is ammonium chloride synthesis schematic diagram.
Fig. 4 is the technological condition figure that the continuous ammonification of 2,4-dinitraniline of the present invention is produced.
Fig. 5 is 2,4-dinitraniline of the present invention continuous ammonification production ammonification segment process and instrument schema.
Fig. 6, Fig. 7, Fig. 8 are the partial enlarged drawings of Fig. 5.
Fig. 9 is that evaporator section process and instrument dia-is produced in the continuous ammonification of 2,4-dinitraniline of the present invention.
Figure 10, Figure 11, Figure 12 are the partial enlarged drawings of Fig. 9.
In Fig. 2, Fig. 3, Fig. 5, Fig. 9, volume pump pump (pressure is at 1.5 ~ 2.5Mpa) is passed through by storage tank after dinitrochlorobenzene fusing, directly deliver to ammonification machine, also use volume pump (pressure is at 1.5 ~ 2.5Mpa) that ammoniacal liquor and condenser are sent into ammonification machine respectively simultaneously, at pressure 0.5 ~ 1Mpa, temperature is aminating reaction under the condition of 160 DEG C ~ 170 DEG C, completes the reaction of more than 99%, enter ripe machine, react more than 99.8%.Again by variable valve floating tank liquid level, flow into cooler decrease temperature and pressure to less than 70 DEG C after keeping the pressure of main reaction machine and ripe machine, then enter separating, washing and centrifugal dewatering.Centrifugal go out 2,4-dinitraniline mother liquor pump delivery is to rapid steamer, temperature 80 DEG C ~ 90 DEG C, vacuum overbottom pressure be the condition of below 0.05Mpa under evaporation concentration, cooling down, crystallization in ammonium chloride cooler is delivered to after concentrated, material after crystallization is transported to whizzer and carries out centrifugation, obtains ammonium chloride product and ammonium chloride mother liquor, and ammonium chloride mother liquor flows into ammonium chloride mother liquor storage tank, use ammonium chloride mother liquor pump delivery to rapid steamer again, continue evaporation concentration.
Embodiment
Below in conjunction with drawings and Examples, further explanation is explained to this patent.But the protection domain of this patent is not limited to concrete embodiment.
The embodiment of this patent, the structure of its main reactor is: 3 charging openings are on the end socket of reactor upper end, discharge port is at the upper end-face edge place of reactor side cylindrical shell, rinse mouth is established in bottom, reactor has agitator, machine envelope and step-down gear, wherein agitator is made up of tubular shaft and double-suction head closed type turbine stirring arm, tubular shaft upper and lower opening, makes the gaseous phase materials above reactor and below stir opening UNICOM.Double-suction head closed type turbine stirring arm structure is: arrange two pieces of circular cover plates respectively in the disc turbine agitator top and bottom meeting HG/T3796.5-2005 that the backward inclined type of impeller by 8 standards forms, open 10-20 the circular hole passed in tubular shaft at agitator axle sleeve position, stirring rake lower end position is provided with current stabilization ring.Auxiliary reactor is usual pressure reactor, its charging opening is 1/10th places of barrel lenght from the distance of end socket in kettle upper end, auxiliary reactor side, export in the upper end of auxiliary reactor side cylindrical shell from 1/9th places that the distance of end socket is barrel lenght, this two places opening angle in the vertical direction upper angle is 90 degree, rinse mouth is established in bottom, auxiliary reactor there is agitator, machine envelope and step-down gear.The stirring of auxiliary reactor is pusher stirring.
Embodiment 1
Main reaction machine, adopt the self-priming turbine stirring of High Temperature High Pressure, agitator is made up of tubular shaft and double-suction head closed type turbine stirring arm, tubular shaft upper and lower opening, makes the gaseous phase materials above reactor and below stir opening UNICOM.Double-suction head closed type turbine stirring arm structure is: arrange two pieces of circular cover plates respectively in the disc turbine agitator top and bottom meeting HG/T3796.5-2005 that the backward inclined type of impeller by 8 standards forms, 10-20 the circular hole passed in tubular shaft is opened at agitator axle sleeve position, stirring rake lower end position is provided with current stabilization ring, first to fill after material increasing temperature and pressure continuous seepage again, eliminate feed time.The design of main reactor designs according to there being gas to participate in the feature of reaction, and be that throughput is large, power consumption is low.
Embodiment 2
Utilize hot water pump to add water to coil pipe in main reactor, thus to main reactor cooling, the temperature of main reactor is controlled at 160 DEG C ~ 170 DEG C.Hot water out becomes steam afterwards from main reactor coil pipe, after steam is collected by sub-cylinder, for evaporation concentration section rapid steamer.Phlegma after evaporative condenser again collect return hot water pump continue cooling to main reactor utilize.The aminating reaction heat that DNFB is one kilogram is 2685.6097KJ/Kg.
(1) the condition required
1. temperature of reaction 165 DEG C
2. pressure 10kg/cm3,
(2) heat brought into by raw material
Heat brought into by table 1 raw material
(3) reaction heat
Q is anti-=1145.75 × 2685.6097=3077037.31KJ/t
(4) the heat taken away of product
The heat that table 2 product is taken away
(5) ammonification thermal equilibrium
The trans-Q one-tenth=328563.32+3077037.31-3151356.88=254243.75KJ/t of the former+Q of Q=Q
Also needing to lead away heat after product reaction per ton is 254243.75KJ/t.So product per ton removes heat radiation and falls 10% heat, and product per ton can produce the use of steam for evaporator section of the heat of 228819.375KJ.
Embodiment 3
Dinitraniline and ammonia react, yield 99%, drop into dinitrochlorobenzene 1145.75kg, after reaction, obtain dinitraniline: 105.48kg, unreacted dinitrochlorobenzene is 5.73kg, the dinitraniline 5.13kg that ripe machine reaction produces, the dinitraniline 5.13+1020.36=1025.49kg of ripe machine, obtains dinitraniline 1025.48 × 0.985=1010.11kg after washing, obtains dinitraniline 1010.11 × 0.99=1000.00kg after filtration.Drop into ammoniacal liquor, ammonia content is 17 ~ 18%, calculate by 18%, it is 201.94kg that reaction drops into ammonia, ask ammonia vol, 201.94 ÷ 0.18=1121.89kg/t, ammoniacal liquor proportion 0.935, volume is 1138.80kg/t, the ammonia of dinitraniline is 1145.75 ÷ 202.55 × 17=96.16kg/t, and the HCl of generation is 1145.75 ÷ 202.55 × 36.5=206.47kg/t, ammonia 206.47 ÷ 36.5 × 17=96.16kg/t that HCl reacts away, remaining ammonia 201.94-96.16-96.16=9.62kg/t, the growing amount 206.47 ÷ 36.5 × 53.5=302.63kg/t of ammonium chloride.
Embodiment 4
As shown in Figure 1, the one 2 of this patent, the continuous ammonification production technique of 4-dinitraniline, adopt 2,4-dinitrochlorobenzene, mass concentration be 18% ammoniacal liquor be raw material, DNFB and 18% ammoniacal liquor mass ratio are 1:1.89, main reaction still controls at 160 DEG C ~ 170 DEG C, and pressure-controlling is at 0.5 ~ 1MPa.
Embodiment 5
By 2,4-dinitrochlorobenzene volume pump scale is adjusted to 2176kg/h, 18% ammoniacal liquor volume pump scale is adjusted to 4110kg/h, phlegma scale is adjusted to 1240kg/h, with volume pump, two kinds of raw materials are continuously added main reactor by reactor charging opening, the charging opening of this reactor is at the end socket position of reactor.Along with main reactor material liquid level rises steadily, after exceeding ammonification machine discharge port, material is successively from flowing to two auxiliary reactors, and by regulating reacting kettle jacketing steam temperature of reaction to be controlled to be 160 DEG C ~ 170 DEG C, it is 0.5 ~ 1.0Mpa that reaction pressure controls.
Reacted material keeps the pressure of main reaction machine and ripe machine by variable valve floating tank liquid level simultaneously, flow into cooler and carry out cooling row pressure, temperature is reduced to 60 ~ 70 DEG C, pressure reduces to normal pressure, form solid-liquid mixture, solid-liquid mixture, after centrifuge washing, enters wrapping machine and carries out finished product packing.
Claims (6)
1. one kind 2, the continuous ammonification production technique of 4-dinitraniline, with DNFB, ammoniacal liquor for raw material, generate 2,4-dinitraniline, it is characterized in that: with volume pump, DNFB, 18% ammoniacal liquor, water of condensation three kinds of raw materials are added reactor and continuously add main reactor by main reactor charging opening, wherein, the add-on of ammoniacal liquor and water makes DNFB: the NH contained in ammoniacal liquor
3mol ratio=1:(3.8 ~ 4.5 of amount), and NH
3: quality ratio=1:(4.3 ~ 4.6);
Main reactor is aminating reaction still, and aminating reaction still adopts the self-priming turbine stirring of double-suction head; According to the volume determination feed rate of main reactor, average residence time of material is made to be 35-50 minute; Temperature 160 DEG C ~ 170 DEG C, pressure reacts under 0.5MPa ~ 1.0MPa condition;
After main reactor material exceedes the discharge port of aminating reaction still, material flow at least the first auxiliary reactor successively certainly, the second auxiliary reactor reacts; The mean residence time of material in every platform auxiliary reactor is 15 minutes; The number of auxiliary reactor is determined according to material reaction speed;
Utilize hot water pump to add water to coil pipe in main reactor, thus to main reactor cooling, make the temperature of main reactor control at 160 DEG C ~ 170 DEG C; Hot water out becomes steam afterwards from main reactor coil pipe, after steam is collected by sub-cylinder, for evaporation concentration section rapid steamer; Phlegma after evaporative condenser again collect return hot water pump continue cooling to main reactor utilize;
The temperature of reaction of two auxiliary reactors is controlled to be 160 DEG C ~ 170 DEG C, by the variable valve after surge tank, reaction pressure is controlled to be 0.5 ~ 1.0MPa, reacted material is through cooling row pressure, temperature is reduced to 60 ~ 70 DEG C, pressure reduces to normal pressure, form solid-liquid mixture, solid-liquid mixture is after centrifuge washing, and solid materials enters wrapping machine and carries out finished product packing.
2. according to claim 12, the continuous ammonification production technique of 4-dinitraniline, it is characterized in that: the structure of described aminating reaction still is: the agitator of aminating reaction still is made up of tubular shaft and double-suction head closed type turbine stirring rake, tubular shaft upper and lower opening, makes the gaseous phase materials above reactor and below stir opening UNICOM; Double-suction head closed type turbine stirring rake by two groups of back-to-back combinations of closed type turbine agitator together, is opened multiple circular hole passed in tubular shaft at agitator axle sleeve position, stirring rake lower end position is provided with current stabilization ring.
3. according to any one of claim 1 or 22, the continuous ammonification production technique of 4-dinitraniline, it is characterized in that: after centrifugal 2, 4-dinitraniline mother liquor adds in rapid steamer, temperature 80 ~ 90 DEG C, vacuum overbottom pressure is evaporation concentration under the condition of below 0.05Mpa, aminating reaction is reused for by collecting in water evaporates to mist collector in unsaturated ammonium chloride solution, the supersaturation ammonium chloride solution be left in rapid steamer utilizes the density in online Density Measuring Instrument detection rapid steamer, control ammonium chloride relay pump flow by density domination in rapid steamer at 1.0 ~ 1.1g/ml, utilize ammonium chloride relay pump by 2, 4-dinitraniline mother liquor is delivered to cooling down in ammonium chloride cooler, crystallization, material after crystallization is transported to whizzer and carries out centrifugation, obtain ammonium chloride product and the ammonium chloride mother liquor containing a small amount of ammonium chloride.
4. according to any one of claim 1 or 22, the continuous ammonification production technique of 4-dinitraniline, it is characterized in that: the structure of described auxiliary reactor is: the charging opening of auxiliary reactor is 1/10th places of barrel lenght from the distance of end socket in kettle upper end, auxiliary reactor side, export in the upper end of auxiliary reactor side cylindrical shell from 1/9th places that the distance of end socket is barrel lenght, this charging opening and outlet angle in the vertical direction upper angle are 90 degree, rinse mouth is established in bottom, auxiliary reactor there is agitator, machine envelope and step-down gear; The stirring of auxiliary reactor is pusher stirring, and auxiliary reactor is provided with jacket heat-preservation.
5. according to claim 32, the continuous ammonification production technique of 4-dinitraniline, it is characterized in that: the structure of described auxiliary reactor is: the charging opening of auxiliary reactor is 1/10th places of barrel lenght from the distance of end socket in kettle upper end, auxiliary reactor side, export in the upper end of auxiliary reactor side cylindrical shell from 1/9th places that the distance of end socket is barrel lenght, this charging opening and outlet angle in the vertical direction upper angle are 90 degree, rinse mouth is established in bottom, auxiliary reactor there is agitator, machine envelope and step-down gear; The stirring of auxiliary reactor is pusher stirring, and auxiliary reactor is provided with jacket heat-preservation.
6. the continuous ammonification production technique of 2,4-dinitraniline according to any one of claim 1 or 2, is characterized in that: after the second auxiliary reactor, arrange surge tank.
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| CN107382739A (en) * | 2017-07-31 | 2017-11-24 | 浙江大井化工有限公司 | A kind of production method of 2,4 dinitroaniline |
| CN109045744B (en) * | 2018-08-30 | 2021-04-27 | 山东亚邦化工科技有限公司 | Method and device for continuously and stably preparing acesulfame potassium crystals |
| CN109078359B (en) * | 2018-08-30 | 2020-11-06 | 山东亚邦化工科技有限公司 | Process and device for continuous extraction of acesulfame potassium sulfonated hydrolysate |
| CN110668954A (en) * | 2019-09-24 | 2020-01-10 | 浙江汇翔化学工业有限公司 | Preparation method of 2, 4-dinitroaniline |
| CN113582852A (en) * | 2020-04-30 | 2021-11-02 | 浙江省常山长盛化工有限公司 | Method for producing dinitroaniline |
| CN111635322A (en) * | 2020-06-15 | 2020-09-08 | 杭州迈科瑞科技有限公司 | Method for preparing 2, 4-dinitroaniline by using microreactor |
| CN113511975A (en) * | 2021-06-25 | 2021-10-19 | 宁夏中盛新科技有限公司 | Safe and environment-friendly preparation process of 2, 4-dinitroaniline |
| CN114805082B (en) * | 2022-04-22 | 2024-01-09 | 浙江华亿工程设计股份有限公司 | Method for preparing nitroaniline by continuous convection ammoniation of nitrochlorobenzene |
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